Solid-phase microextraction and gas chromatography-mass spectrometry for quantitative determination of chlordecone in water, plant and soil samples

Abstract

Introduction. Chlordecone (CLD), an organochlorine formerly used to control the banana black weevil, is strongly adsorbed on soils, particularly on andosols. A simplified analytical procedure for the quantitative determination of chlordecone residues in water and micro-samples of soil and plants was compared with a standard method. Materials and methods. The procedure combines a simplified sampling protocol and a 10-min solid phase microextraction (SPME), followed by gas chromatographic separation (GC) and mass spectrometric (MS and MS/MS) identification. Quantitation of CLD used a standard addition method with zero extrapolation. First, seventy samples were analysed using the proposed method and the standard method based on hot solvent extraction. Second, fifteen soil samples were analysed with two SPME methods followed by GC-MS but using CLD labelled with C13 as an internal standard or the proposed method. Results and discussion. The detection (LOD) and quantitation (LOQ) limits of our SPME extraction procedure were determined for GC-MS and GC-MS/MS with water, plant (pineapple roots) and soil samples: in water for MS/MS, LOD MS/MS-water = 0.5 ng⋅L -1 , LOQ MS/MS-water = 2.0 ng⋅L -1 ; in andosol for MS/MS, LOD MS/MS-soil = 15.0 ng⋅kg -1 dw, LOQ MS/MS-soil = 80.0 ng⋅kg -1 dw. Data from the seventy contaminated soils obtained with the proposed method and the standard method showed a correlation coefficient of r = 0.86. Data obtained by the two SPME/GC-MS quantitation procedures showed a correlation of r = 0.8073. Conclusion. The method proposes a simplified sample preparation and extraction of CLD in water, plant and soil samples, with no solvent manipulation and which is not time-consuming. The LOD and LOQ were similar to those obtained with other currently used methods. The method is reli- able and accurate and may be considered as a good tool for research purposes. France (Martinique) / chlordecone / extraction / analytical methods / quantitative analysis / water analysis / soil analysis / tissue analysis